In this research, nanofibers of polymamide 66 containing MgO and nanofibers of polyamide 66 containing Al2O3 nanoparticles were electrospun in order to detoxify 2-chloroethyl ethyl sulfide (2-CEES). The solutions containing 10%, 12% and 14% W/W of polymer and 10%, 12% and 15% of each of nanoparticles in formic acid, were prepared using sonicator, and the effects of sonication and particle concentration on viscosity and electrical conductivity of fluids were investigated. These solutions were electorspun to produce nanofibers. Transmission Electron Microscopy (TEM) was applied to measure the size of nanoparticles and to evaluate the quality of dispersions. TEM was also used to study the distribution and size of nanoparticles in nanofibers. The effects of polymer and nanoparticle concentrations on morphology and average diameter of nanofibers were studied using Scanning Electron Microscope (SEM). FTIR results showed that no chemical reactions between polymer, formic acid and nanoparticles took place. Detoxification of 2-CEES (a mimic of mustard) by each of two nanoparticles was studied using gas chromatography. Afterwards, the ability of nanofibers containing these nanoparticles was studied for detoxification of this toxic chemical. Results indicated that increase in the concentration of MgO and Al 2 O 3 nanoparticles, causes an increase in viscosity and electrical conductivity of fluids. Due to the contradictory effect of viscosity and electrical conductivity by varying the concentration of nanoparticles, there was not any specific trend in the fiber diameter. Our Results also showed that MgO nanoparticles could not detoxify 2-CEES but Al 2 O 3 whiskers had the ability to detoxify 89% of 2-CEES under our experimental conditions. The finest nanofibers containing Al 2 O 3 nanoparticles that was electrospun in this study could reduce 78% of 2-CEES from the reaction medium. Due to about 9% physisorption of 2-CEES by nanofibers, The ability of these nanofibers for detoxification of 2-CEES was calculated about 69%.